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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Chemical mechanisms and kinetic modeling of calcium aluminate cements hydration in diluted systems: Role of aluminium hydroxide formation

Calcium aluminate cements are niche cements used in the refractory industry and in non-structural applications for building chemistry with short return-to-service delay. The later applications use theses cements in combination with calcium sulfates for long-term stability. By being niche cements, the knowledge of calcium aluminate cements hydration is not as extensive as that of Portland cement. In the present paper, the calcium aluminate cements are studied in diluted suspensions as a function of different parameters such as the suspension concentration or the quantity of added calcium sulfates. The objective is to identify their baseline chemical mechanisms. This work demonstrates the essential role of hydroxide ions fluxes, i.e. quantity going in and out of the liquid phase per unit of time. The main quantitative flux is the formation of aluminium hydroxide but the activation of this reaction is difficult. This difficulty allows calcium aluminate to be used as cement by creating a dormant period (workability) for the overall reactivity. The identification of the key role of aluminium hydroxide formation explains the influence of the temperature, some mechanisms of setting admixtures and the early age of calcium aluminate cements.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Experimental and theoretical study of the restrained shrinkage cracking of early age well cement

The shrinkage cracking occurring in oil & gas well cement material is a major factor that reduces the cement sheath integrity and impairs the durability of an underground well. Shrinkage mainly takes place in the early hydration period of the cement, and the resulting restrained shrinkage cracking can form a leaking network for oil & gas or carbon dioxide stored in an underground reservoir. It is thus important to understand the early age behavior of well cement and the leaking pathway formation in the well. This study describes the application of the digital image correlation (DIC) method as a tool to measure the strain development and crack distributions of well cement in the lab during early phase changes. A theoretical model is presented to calculate the stress distribution built up in the cement sheath during early ages of well cement hydration, which helps to interpret the experimental observations and determine the major factors influencing the cracking sequences. This study presents the whole hydration – drying shrinkage – and cracking mechanism of early age well cement under restrained ring conditions experimentally and theoretically. Finally, the results offer useful insights on the key material and geometric parameters which control the fracture of a well cementing structure.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Thermal shock resistance of lightweight cements developed for geothermal conditions

Cements are a critical component in well construction, as they act to prevent well fluid and gas escape, prevent corrosion of the casing, and strengthen the wellbore to prevent deformation. Under the high temperature/pressure conditions common in geothermal systems, the injection of cold water for energy production is expected to induce cyclic damage to the borehole cement through the rapid temperature fluctuations. These “thermal shocks” are expected to cause casing shrinkage, annulus formation, and cement tensile stresses. To understand the effect of cold water injection on the wellbore environment, a set of rock-cement-steel samples were created to simulate the structure of a geothermal well. Lightweight thermally-insulating cement blends were tested under thermal shock conditions in this study. In each test, the samples were pressurized to an effective pressure of ~3.5 MPa and placed at high temperatures. Thermal shocks were performed by injecting cold water (~10-15 °C) through the samples at a constant rate while keeping the samples at high temperatures until the sample temperature stopped decreasing and deformation ceased. Eight thermal shock tests were conducted with each sample – two at 100 °C and six at 200 °C. Post-tests analysis was then conducted by cutting open each sample to examine the damage in each component of the simulated wellbore. Experimental results suggest that all samples experienced similar degrees of axial and lateral contraction during cold water injection, but for the most part this contraction is recoverable when injection halts. Post-test analysis revealed that fly ash cenosphere pre-treatment had the best effect on improving thermal shock resistance in the cement blends. Thermomechanical modeling of likely stress paths experienced by the cements during heating/cooling cycles shows that elasto-plastic cement constitutive behavior results in most plastic strain occurring during the initial heating steps, with mostly elastic strain occurring during the thermal shock cycles. In conclusion, this agrees with experimental evidence, suggesting that cement damage from shocking occurs via other mechanisms such as chemical alteration, corrosion, and fatigue.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Sulfate Promotes Compact CaCO 3 Formation and Protects Portland Cement from Supercritical CO 2 Attack

Supercritical (sc) CO 2 in geologic carbon sequestration (GCS) can chemically and mechanically deteriorate wellbore cement, raising concerns for long-term operations. In contrast to the conventional view of “sulfate attack” on cement, we found that adding 0.15 M sulfate to the acidic brine can significantly reduce the impact of scCO 2 attack on Portland cement, resulting in stronger cement than that found in a sulfate-free system. Scanning electron microscopy revealed a decreased total attack depth in reacted cement in the presence of sulfate. With a newly defined minimum porosity term in reactive transport modeling, our model suggests that sulfate caused CaCO 3 to fill more nanopore spaces in the cement. Small angle X-ray scattering experiments also showed that sulfate can decrease the pore sizes of the carbonate layer. The results suggest that the interactions between sulfate and cement can generate a less porous CaCO 3 layer, which better resists acidic brine. Using this mechanism as a proof-of-concept, we tested the incorporation of sodium sulfate into Portland cement and synthesized new cement composites that show stronger resistance against scCO 2 attacks. Finally, these newly discovered interfacial interactions between CaCO 3 and sulfate provide new insights into engineering mechanically strong and green materials for safer GCS.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Laboratory Foamed-Cement-Curing Evolution Using CT Scanning: Insights From Elevated-Pressure Generation

Computed-tomography (CT) scanning has become a mainstay among scientists (Wildenschild and Sheppard 2013) because it enables nondestructive observation of material processes and formation in real time. Foamed cement is a high-strength, low-density material containing nitrogen gas, and is used to stabilize wellbore casings both onshore and offshore. In-situ foamed cement is subject to pressure changes because the slurry is pumped downhole and cures at depth. To correlate the influence of pressure to the gas-void size and the curing evolution of a foamed cement, two laboratory foamed cements were generated and CT scanned as they cured. One cement was generated following the American Petroleum Institute (API) industry standard API RP 10B-4 (2015) at atmospheric conditions using a blender, and the other cement was created using a foamed-cement generator (FCG) (resembling that of de Rozières and Ferrière 1991) to produce a sample at an elevated pressure. FCG-generated cement qualities (in the range of 20, 25, 30, 35, and 40%) were scanned at their cured state for comparison. From the CT-image time series and the single FCG scans, the volumetric void properties were characterized and compared. The time-series blender voids were an order of magnitude larger than the FCG voids, and void growth was stagnant after a curing period of 100 minutes, whereas the FCG voids gradually increased in volume after 100 minutes. The Hsü-Nadai plots (Brandon 1995) reveal that the FCG and blender voids are weakly prolate, and all FCG voids, regardless of generation quality, relax to a greater final-magnitude strain than the blender voids. Furthermore, these findings confirm that both the void size and the curing process are influenced by the pressure at which a foamed cement is generated.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Advanced Self-Healing Polymer-Cement Composites for Geothermal Wellbore Application at 300 °C

Polymer-cement composites were formulated using two base cements and three polymers and evaluated as potential alternatives to conventional geothermal wellbore cementitious material. To mimic geothermal conditions these cement composites were cured at 300 °C and their mechanical properties, including compressive strength, Young modulus, shear bond strength to steel casing, and self-healing and re-adhering (to steel) capability were tested. To test thermal stability the samples were cured at 300 °C for up to 30 days followed by analysis of their mineralogy and chemical composition by X-ray diffraction spectroscopy (XRD), 13C NMR, and total organic carbon (TOC). These tests showed that all polymer composites formulated were thermally stable as supported by almost 100% TOC of the 300 ?C cured samples and presence of all the polymer signals in 13C NMR permeability tests performed before and after healing a longitudinal fracture base cements and polymer-cement composites gave lower (2nd/1st) permeability ratios with respect to base cements which suggests that introduction polymers result in self-healing composite materials. Curing two of the best performing polymer-cement composites for a period of 30 days at 300 °C maintained the self-healing capability. These advanced polymer-cement composites with higher mechanical stability, ductility and self-healing capability are promising alternatives to wellbore cement materials for geothermal and fossil energy applications.

polymer-cement, composite, wellbore, self-healing,↗
DOE OSTI2017

Polymer-Cement Composites with Self-Healing Ability for Geothermal and Fossil Energy Applications

Sealing of wellbores in geothermal and tight oil/gas reservoirs by filling the annulus with cement is a well-established practice. Failure of the cement as a result of physical and/or chemical stress is a common problem with serious environmental and financial consequences. Numerous alternative cement blends have been proposed for the oil and gas industry. Most of these possess poor mechanical properties, or are not designed to work in high temperature environments. This work reports on a novel polymer-cement composite with remarkable self-healing ability that maintains the required properties of typical wellbore cements and may be stable at most geothermal temperatures. We combine for the first time experimental analysis of physical and chemical properties with density functional theory simulations to evaluate cement performance. The thermal stability and mechanical strength are attributed to the formation of a number of chemical interactions between the polymer and cement matrix including covalent bonds, hydrogen bonding, and van der Waals interactions. Self-healing was demonstrated by sealing fractures with 0.3–0.5 mm apertures, 2 orders of magnitude larger than typical wellbore fractures. This polymer-cement composite represents a major advance in wellbore cementing that could improve the environmental safety and economics of enhanced geothermal energy and tight oil/gas production.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Oil and gas flow through fractures and along interfaces in well cement

A number of wells at the Strategic Petroleum Reserve (SPR) have shown sustained, positive pressure (referred to as sustained casing pressure or SCP) in the cemented annulus behind the production casing. To better understand how SCP may develop for SPR conditions, we conducted gas and oil flow tests on cement specimens with flaws including cement fractures and discrete interfaces along a cement-steel contact. Many specimens were tested initially with gas, followed by oil, and finally with gas again to identify how the fluid type may affect the flow through flaws in the well cement. Nitrogen was used as the gas, and silicone oil with properties similar to typical crude oil was used in most tests. One set of measurements were made with crude oil. Composite steel-cement specimen with corroded steel were also tested. For both gas and oil tests, the measured flow test data were used to interpret permeability and, assuming the cubic law for flow between parallel plates, the corresponding hydraulic aperture of the flaw. The hydraulic apertures for the flawed specimens ranged from about 20 to >100 μm, which corresponds to permeabilities of about 10 -14 to 10 -12 m 2 , respectively; these hydraulic apertures are consistent with the range of values interpreted from field measurements on leaky wells. Observed differences between the flow of gas and oil were attributed to a number of factors, including non-linear flow of gas, possible blocking of flow paths by solids within the crude oil, two-phase gas and oil flow and the presence of residual oil in the cement flaw. Furthermore, we determined that corroded steel itself is permeable. Using input values consistent with the gas and oil flow measurements, we conducted one-dimensional simulations of gas and oil flow through cemented annulus systems to investigate the role of flaw size and fluid type on the expected response (i.e., pressure build-up) in the annular cement.

02 PETROLEUM↗
DOE OSTI2021

DPC Cement Filler Development (Progress Report)

The fillers research and development (R&D) program, mostly experimental, is part of a broader R&D program that includes new process modeling and performance assessment of criticality effects and the overall importance of criticality to repository performance (consequence screening). A literature research and consultation effort with experts by Hardin and Brady (2018) identified several potentially effective and workable filler materials including cements (primarily phosphate based), moltenmetal alloys, and low-temperature glasses. Filler attributes were defined, and the preliminary lists were compared qualitatively. Further comparative analysis will be done (e.g., cost estimates) after experimental screening has narrowed the list of alternatives. The following cement filler compositions were selected for experimental development work and accelerated testing in FY20: Aluminum phosphate cements (APCs); more specifically aluminum oxide / aluminum phosphate (Al 2 O 3 / AlPO 4 ) cements in which Al 2 O 3 serves as the filler material bound by an AlPO 4 binder formed by the reaction of Al 2 O 3 with H 3 PO 4 ; Calcium phosphate cements (CPCs); more specifically composed of pure or nearly pure hydroxyapatite or HAP (Ca 5 (PO 4 ) 3 (OH)); Wollastonite phosphate cements (WPC), specifically wollastonite and aluminum or calcium aluminum phosphates in which CaSiO 3 serves as the filler material and the phosphate serves as the binder. The FY20 effort focused on the optimization of compositions and subsequent processing of these three materials to achieve dense and well-consolidated monolithic samples with 30 to 40% porosity and permeabilities of 1 millidarcy. At the close of this progress report the aluminum phosphate cements (APCs) and the wollastonite phosphate cements (WPCs) appear to show the most promise for continued development. Less progress has been made with the calcium phosphate cements (CPCs); their slurry viscosities are high (and difficult to measure) and they exhibit relatively short cure times of 2 to 3 hours with concomitant and excessive volatile (e.g. CO 2 ) generation.

36 MATERIALS SCIENCE↗
NASA NTRS2009

A Model of Thermal Conductivity for Planetary Soils: Theory for Cemented Soils - 2

A numerical model of heat conduction through particulate media made of spherical grains cemented by various bonding agents is presented. The pore-filling gas conductivity, volume fraction, and thermal conductivity of the cementing phase are tunable parameters. Cement fractions <0.001-0.01% in volume have small effects on the soil bulk thermal conductivity. A significant conductivity increase (factor 3-8) is observed for bond fractions of 0.01 to 1% in volume. In the 1 to 15% bond fraction domain, the conductivity increases continuously but less intensely (25-100% conductivity increase compared to a 1% bond system). Beyond 15% of cements, the conductivity increases vigorously and the bulk conductivity rapidly approaches that of bedrock. The composition of the cements (i.e. conductivity) has little influence on the bulk thermal inertia of the soil, especially if the volume of bond <10%. These results indicate that temperature measurements are sufficient to detect cemented soils and quantify the amount of cementing phase, but the mineralogical nature of the bonds and the typical grain size are unlikely to be determined from orbit. On Mars, a widespread surface unit characterized by a medium albedo (0.19-0.26) and medium/high thermal inertia (200-600 J s(0.5)/sq m/K) has long been hypothesized to be associated with a duricrust. The fraction of cement required to fit the thermal data is less than approx.1-5% by volume. This small amount of material is consistent with orbital observations, confirming that soil cementation is an important factor controlling the thermal inertia of the Martian surface

Piqueux, S.↗
DOE OSTI2019

Shelf life of alkali activated cement: Effects of storage condition and duration

Hydraulic cements based on the alkali aluminosilicate chemistry tend to be more reactive than Type I Portland cement. An experimental investigation was conducted in order to evaluate the effects of storage in air and in sealed condition on the properties and performance of alkali aluminosilicate cements. Different storage durations up to 28 days were considered in this experimental study. Hydraulic cements were evaluated based on their morphology, chemistry and mineralogy, hydration kinetics, strength development characteristics, and microstructure of the resultant hydration products. The early-age hydration kinetics and strength development characteristics of the alkali aluminosilicate cement were found to be altered by storage, especially when the cement was exposed to air. Older cements also produced hydration products that were more susceptible to microcracking when dried under vacuum. Longer-term strength development characteristics of cements were less influenced than their shorter-term strength development characteristics with duration of storage in sealed or exposed condition.

36 MATERIALS SCIENCE↗
DOE OSTI2024

State of Innovation 2024: Paving the Way for Low-Carbon Cement and Concrete

Concrete production in the U.S. accounted for nearly 393 million cubic yards in 2023, with $38.8 billion in revenue. While cement, the key ingredient in concrete, is only 10%-15% of concrete's mixture by mass, 8% of total global emissions come from the production of cement. A significant challenge lies in the fact that roughly 51% of concrete emissions stem from the material calcination process of cement production. Stakeholders ranging from cement producers to government agencies are beginning to take measures to significantly reduce concrete emissions by 2050 and are seeking novel technologies from the startup community. Strategies to lower carbon emissions include reducing quantities of cement in concrete formulas; optimizing digital and automated production; lower temperature processing; carbon capture, utilization, and durable storage; and other cost-saving approaches to energy and material efficiencies. New materials based on carbon mineralization and novel cement chemistries hold the potential to reach net-zero or even carbon-negative concrete production; however, there is presently no readily available substitute that can replicate concrete's unique properties and versatility at the volume demanded by construction worldwide. The nature of concrete's raw materials, diverse applications, and scale of demand means that complete decarbonization will rely on a combination of innovative production methods and novel cement chemistries. Low-carbon solutions will need to compete economically with traditional concrete to become viable in a high-volume commodity market, although consumer demand and regulation will play important roles. Despite these challenges, this analysis reveals that venture capital (VC) investments in low-carbon concrete reflect a growing awareness of the decarbonized cement market opportunity. Between 2022 and 2023 emerging low-carbon technologies garnered more than $700 million in VC investments, representing a growing share of investment in the built environment. An investment gap appears after Series A for technology solutions, demonstrating the sector's potential, as well as the need for additional performance assurance and technology incubation.

cement↗
DOE OSTI2026

Discovery of nanopore filling by gypsum in wellbore cement exposed to 17 MPa CO 2 under geologic carbon storage conditions

Here, this study investigates the pore structure evolution of the reaction zones in wellbore cement samples exposed to a CO 2 -rich solution in equilibrium with 17 MPa supercritical CO 2 over 14 days. Through advanced characterization methods of field emission SEM, Quantitative Evaluation of Minerals by Scanning Electron Microscopy (QEMSCAN), and micro-CT, a new mechanism of CO 2 -cement reaction involving filling of nanopores in the interior of cement by gypsum was revealed. Gypsum was formed by the liberation of SO 4 2− from ettringite (AFt) and monosulfate (AFm) caused by a decrease in pH. Based on these experimental observations, a new CO 2 -cement reaction model that incorporates four distinct reaction zones is developed. This model provides a comprehensive framework for understanding the spatial and temporal distribution of minerals in cement due to high pressure CO 2 —cement reactions. This study demonstrates that the major damage induced by high pressure CO 2 alteration occurs in the most exterior region of the cement. The interior region of the cement maintains its integrity due to nanopore filling by gypsum.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

The mechanisms, dynamics, and implications of self-sealing and CO 2 resistance in wellbore cements

Here, this study analyzes the dynamics and mechanisms of the interactions of carbonated brine with hydrated-Portland-cement; in particular, the study focuses on self-sealing, a process whereby hydrated-Portland cement reacts with carbonated brine to for silica and calcium carbonate in sufficient quantities to seal the flow pathway. The analysis is based on a comprehensive set of reactive-transport simulations that explore the complex coupled dynamics between the fluid flow and mineral reactions that underlie self-sealing, and it relies heavily on the synthesis of the extensive body of work on wellbore integrity that has been conducted over the past decade. The analysis explores a large chemical and mineralogical diversity and a wide range in physical conditions and flow regimes, attempting to assess the robustness of the analysis. Self-sealing conditions arise over a wide range in cement properties and reservoir conditions. Although some properties and conditions promote a stronger self-sealing response, self-sealing occurs for a wide range of Ca:Si ratios in cement and for various reservoir fluid compositions. Self-sealing conditions move along a wellbore proportional to the flux of the leaking carbonated brine, and the reaction zone spreads out proportional to the fluid velocity, where volumetric flux and velocity are related by porosity (flux = velocity * porosity). However, self-sealing conditions can be maintained in a specific section of a wellbore by controlling the pressure drive and/or effective wellbore permeability, which in turn can limit the flux and velocity of any leaking fluid. Finally, the phases produced by hydrating Portland cement represent a carbonic cement that will react with a carbonated brine to produce end products (calcium carbonate and silica) that can maintain integrity in the presence of carbonic acid. Lastly, the attributes that make hydrated Portland cement phases a carbonic cement are required for self-sealing.

58 GEOSCIENCES↗
DOE OSTI2023

Testing Various Cement Formulations under Temperature Cycles and Drying Shrinkage for Low-Temperature Geothermal Wells

Low-enthalpy geothermal wells are considered a sustainable energy source, particularly for district heating in the Netherlands. The cement sheath in these wells experiences thermal cycles. The stability of cement recipes under such conditions is not well understood. In this work, thermal cycling experiments for intermediate- and low-temperature geothermal well cements have been conducted. The samples were cured either under ambient conditions or under realistic pressure and temperature for 7 days. The samples did not show any signs of failure after performing 10 cycles of thermal treatment between 100 °C and 18 °C. We also tested cement formulations under drying conditions. Drying shrinkage is caused by a reduction in the water content of cement, which leads to capillary forces that can damage cement. Such circumstances lead to tensile stresses causing radial cracks. Most samples exhibited cracks under low humidity conditions (drying). Fiber reinforcement, especially using short PP fibers, improved the cement’s resilience to temperature and humidity changes. Such additives can improve the longevity of cement sheaths in geothermal wells.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Environmental Performance Analysis of Cement Production with CO 2 Capture and Storage Technology in a Life-Cycle Perspective

Cement manufacturing is one of the most energy and CO 2 intensive industries. With the growth of cement production, CO 2 emissions are increasing rapidly too. Carbon capture and storage is the most feasible new technology option to reduce CO 2 emissions in the cement industry. More research on environmental impacts is required to provide the theoretical basis for the implementation of carbon capture and storage in cement production. In this paper, GaBi software and scenario analysis were employed to quantitatively analyze and compare the environmental impacts of cement production with and without carbon capture and storage technology, from the perspective of a life-cycle assessment; aiming to promote sustainable development of the cement industry. Results of two carbon capture and storage scenarios show decreases in the impacts of global warming potential and some environmental impacts. However, other scenarios show a significant increase in other environmental impacts. In particular, post-combustion carbon capture technology can bring a more pronounced increase in toxicity potential. Therefore, effective measures must be taken into account to reduce the impact of toxicity when carbon capture and storage is employed in cement production. CO 2 transport and storage account for only a small proportion of environmental impacts. For post-combustion carbon capture, most of the environmental impacts come from the unit of combined heat and power and carbon capture, with the background production of MonoEthanolAmine contributing significantly. In combined heat and power plants, natural gas is more advantageous than a 10% coal-saving, and thermal efficiency is a key parameter affecting the environmental impacts. Future research should focus on exploring cleaner and effective absorbents or seeking the alternative fuel in combined heat and power plants for post-combustion carbon capture. If the power industry is the first to deploy carbon capture and storage, oxy-combustion carbon capture is an excellent choice for the cement industry.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Thermally Insulating, Thermal Shock Resistant Calcium Aluminate Phosphate Cement Composites for Reservoir Thermal Energy Storage

This paper presents the use of hydrophobic silica aerogel (HSA) and hydrophilic fly ash cenosphere (FCS) aggregates for improvements in the thermal insulating and mechanical properties of 100- and 250 °C-autoclaved calcium aluminate phosphate (CaP) cement composites reinforced with micro-glass (MGF) and micro-carbon (MCF) fibers for deployment in medium- (100 °C) and high-temperature (250 °C) reservoir thermal energy storage systems. The following six factors were assessed: (1) Hydrothermal stability of HSA; (2) Pozzolanic activity of the two aggregates and MGF in an alkali cement environment; (3) CaP cement slurry heat release during hydration and chemical reactions; (4) Composite phase compositions and phase transitions; (5) Mechanical behavior; (6) Thermal shock (TS) resistance at temperature gradients of 150 and 225 °C. The results showed that hydrophobic trimethylsilyl groups in trimethylsiloxy-linked silica aerogel structure were susceptible to hydrothermal degradation at 250 °C. This degradation was followed by pozzolanic reactions (PR) of HSA, its dissolution, and the formation of a porous microstructure that caused a major loss in the compressive strength of the composites at 250 °C. The pozzolanic activities of FCS and MGF were moderate, and they offered improved interfacial bonding at cement-FCS and cement-MGF joints through a bridging effect by PR products. Despite the PR of MGF, both MGF and MCF played an essential role in minimizing the considerable losses in compressive strength, particularly in toughness, engendered by incorporating weak HSA. As a result, a FCS/HSA ratio of 90/10 in the CaP composite system was identified as the most effective hybrid insulating aggregate composition, with a persistent compressive strength of more than 7 MPa after three TS tests at a 150 °C temperature gradient. This composite displayed thermal conductivity of 0.28 and 0.35 W/mK after TS with 225 and 150 °C thermal gradients, respectively. These values, below the TC of water (TC water = 0.6 W/mK), were measured under water-saturated conditions for applications in underground reservoirs. However, considering the hydrothermal disintegration of HSA at 250 °C, these CaP composites have potential applications for use in thermally insulating, thermal shock-resistant well cement in a mid-temperature range (100 to 175 °C) reservoir thermal energy storage system.

58 GEOSCIENCES↗
DOE OSTI2018

Deciphering mineralogical changes and carbonation development during hydration and ageing of a consolidated ternary blended cement paste

To understand the main properties of cement, a ubiquitous material, a sound description of its chemistry and mineralogy, including its reactivity in aggressive environments and its mechanical properties, is vital. In particular, the porosity distribution and associated sample carbonation, both of which affect cement's properties and durability, should be quantified accurately, and their kinetics and mechanisms of formation known both in detail and in situ . However, traditional methods of cement mineralogy analysis ( e.g. chemical mapping) involve sample preparation ( e.g. slicing) that can be destructive and/or expose cement to the atmosphere, leading to preparation artefacts ( e.g. dehydration). In addition, the kinetics of mineralogical development during hydration, and associated porosity development, cannot be examined. To circumvent these issues, X-ray diffraction computed tomography (XRD-CT) has been used. This allowed the mineralogy of ternary blended cement composed of clinker, fly ash and blast furnace slag to be deciphered. Consistent with previous results obtained for both powdered samples and dilute systems, it was possible, using a consolidated cement paste (with a water-to-solid ratio akin to that used in civil engineering), to determine that the mineralogy consists of alite (only detected in the in situ hydration experiment), calcite, calcium silicate hydrates (C-S-H), ettringite, mullite, portlandite, and an amorphous fraction of unreacted slag and fly ash. Mineralogical evolution during the first hydration steps indicated fast ferrite reactivity. Insights were also gained into how the cement porosity evolves over time and into associated spatially and time-resolved carbonation mechanisms. It was observed that macroporosity developed in less than 30 h of hydration, with pore sizes reaching about 100–150 µm in width. Carbonation was not observed for this time scale, but was found to affect the first 100 µm of cement located around macropores in a sample cured for six months. Regarding this carbonation, the only mineral detected was calcite.

36 MATERIALS SCIENCE↗